Apparatus for treating lignocellulose.



G. H. ToMLINsoN.

APPARATUS FOR TREATING LIGNO GBLLULOSE.

V I APPLICATION FILED JAN.29,191Z. L032A49.

Patented July 16, 1912.

4 sHBBT-SHBET 1.

G. H. TOMLINSON. APPARATUS FOR TREATING LIGNO GELLULOS.

APPLICATION FILED JAN.29,1912.

Patented July 16, 1912.

4 SHEETS-SHEET 2.

G. H. TOMLNSON.

APPARATUS POR TRBATING LIGNO CELLULOSB. APLIUATION FILED JAN.29,1912.

'PatentedJuly 16, 1912@ 4 SHEETS-SHEET a.

G. H. TOMLINSON.

APPARATUS P011 TRBATING LIGNo -GELLULosBl APBLIOATION FILED JAN.29.1912,

1,032,449. Pantea Ju1y 16, 1912.

4 SHEETS-SHEET A.

iinrrnn s'rAfrns ,learner caricia. y

GEORGE H. 'roi/LLINSON, or CHICAGO. inLrNois, A ssieixion ro STANDARD ALCOHOL COivirANY, or NEWBQRK, N. A CORPORATIONJOF MAINE.'

To al! ywhomA z'z. muy `conce/1% f 'Be 1t known that I." GEORGE H. TorriansoN, a subJec-t ot the King of Great Britain,

residing at Chicago, in the county vof Cook and State oflllinoi-s, -havev invented certain new and useful Improvements inApparatus .tor Treating Lignocellulosdcf which the following is a specification.

This invention relates4 to apparatus `for treating ligne-cellulose orl'other cellulosic raw materials for the purpose ofobtaining turpentine.- or other volatile' products, andl ferinentabjle' sugarsf j For a full understanding of. the invention,v reference is made to the accompanyingy drawings, illustrating a preferred apparatus embodying they invention.

with acid-resisting brick 2, set in a ysuitable, .I 'cement inert to the hydrolyzi-ng agent used. I For use with sulfuric or 'sulfurous acidI -a suitable cement may comprise ami-Xture of litnliargeand glycerin. The liningv shouldI beo't'.` substantial thickness and of a lheatinsulating and" heat-retaining character, in

ordeiithat the charge may be digested by the ai'dj'o'f lire steam admitted to the interior thereof, and the condensation yso limitedl thatthe inass is maintained throughout the ventire operation in an openfpermeable and absorptive-state,as more `fully pointed out in my copending application, Ser. No. 6G4,373tiled Dec. 7,1911.

The digester is provided with a manhole 3 for the introduction and discharge of the material, and with a blow-off cock 4, which in one position of the digester `may he coupled with the blow-olf pipe The digester is mounted' on hollow trunnions (5,.7 and is adapted for rotation by means otl a wormgear 8.

Specification of Letters Patent.`

APPARATUS ron TRATING LioNocELLULosE.

iatented July 16, 1912.

Applicatoirled JanuaryZB, 1912. Serial No. 674,165?.

The .preferred use. ofl the l. apparatus in 55 volves the `introduction of, steamand a hydrolyzingagent. into the ,digesteig andthe withdrawal .of the vapors.therefrom, with-V out-.interrupting its moyement of, rotation.

Connections permitting this-mode of opeia'- 60 tion compiise7 .in the form of apparatus illustrated, a fixed pipe 9 kcitt-ending through.

the lhollow trunnion 6, axially disposed 4within the digester, and perforated as indi-- cated at .lO'for the admission of steanrifto` 65 the interiorl ot the.` charge. j This steam-f pipe is provided vwith a check-valvevll, and

connected with a source o'fsteam'by pipe 1,2, controlled `by a.. Valve .13. Aln practice a plurality ofsimilar dige i ers are vusualy employed, and n'ieansa'ifef .pret'erablyprovided whereby anyA digester ofthe series maybe blown o into otherfdil l gesters which may be in condition tio receive,

the .steam 'oryapors therefrom,l`v For this 75 purpose, I. provide a cond'uitjlM, having vsimilar connections topach digester of the series. illustrated, such connections comprise a. pipe 15, communicating with the steamfinlet pipe 9 at a point between the 80 check-valvell and the control valve 13, by means of the pipe 16 fitted with a valve 17; and likewise lcommunicating through pipe 18, having a'yalvel), with the vapor-eduction pipe 20..;T`his pipe 20 enters the di#` 85 gester through. the hollow tru'nnion 7, and is inalinement with the steainfinlet pipe 9 and is attached thereto by a. Tconnection 21,

.communication between the pipes y9 and .20

beinginterrupted by a blank flange 2Q.

Y T23' is a' Curved 'vaporfeduction pipe, which is carriedby the steam-inlet pipe`-9 and by the -vapor-eduction pipe 20, communicating 'with the latter through "theT 2l, but. sealedy fromt-he pipe 9 by a blank' flange Q4 in the' 95 T ,connection Q5. The pipe Q3 arches upf",

`wardly into the vapor space ofthe' dig'ester, l

and is perforated therein "as indicated 'at .26. As illustrated in Fig.'4 1, and indicated by dotted lines in Fig. 2, the` pipe '23 extends 100 upwardly from the axis yof the digeslcr at van angle of 'approximately 450 from the vertical. The result fthis arrangeineut is that when the digester is'i'otatfl in the direction indicated bythe arrow in Fig. the i05` pipe :23 lies substantially at a right anglcto `the inclined surface of the charge. lt there fore notonly extends to-the maximum dev 'gree into'the vapor space ofthe digester, brit it is subject to the minimum strain-due to` the weight and pressure ofthe charge:l l'

The pipe 2O Vcommunicates at -a point outside the digester with a vapor-pipef27 leading to a suitable condenser 28- for volatile products. In the pipe 27 I place a Valve 29, and around this Valve-I arrange al vvapor'bypass 30, provided with a pop Valve 32, which when 'properly set will serve to 'keep the pressurel uni orm, excessive temperatures- 4 f '.The hydrolyzing agent is introduced into :the dig-ester through 4a Valved pipe 33, which 15 lieswithiii the Vapor-educti in pipes- 20 and 23, and terminates in a spray-nozzle 34,10- cated in the vapor space of the digester and directed toward the surface of the charge theiyzin.

v fA-n 'llusti'ative procedure` when my apparatus is applied t'o the treatment of resinous woods, is as follows: rIhe digester is charged with moistsawdust or wood-waste lto such extent that the steam-inlet pipe 9 is covered, while the perforated portion of the arched eduction-pipe 23 is exposed. gester is then closed and set in' rotation, and Isteam is admitted under suitable pressure to the interior of the charge through the axial, perforated pipe 9, until the/wood is brought to a temperature proper for the distillation of turpentine .or similar volatile products, but below that at which any material decomposition of cellulose occurs, such decomposition at high temperatures resulting, as is well known, in the production of considerable quantities of acetic. acid and tarry and phenolic bodies. v For this purpose, a temf the turpentine and steam will flow through perature not exceeding that of steam under a pressure of twenty to thirty pounds willA usually suffice, and lower pressures may be used 1f desired.. The-valve 29 being opened,

the perforations 26 into the pipe system 23,

20, 27, and thence to the'condenser 2S where the turpentine'and .any accompanying volatile products will be recovered. This'distil'lation `is continued until the elimination of the turpentine is substantially complete.

The steam-supply is then cut off, the educ-` tion-Xalve 29 closed, and the hydrolyzing agent admitted into the digester through the spraj'f-nozzle 34. p

In' the preferred' mode of operation, the hydrolizing agent isl supplied at a tempergatuite materially below that ofthe wood,

lwhich has, by the treatment above described, been brought to a temperature above the Vaporizing point of water. rlhe moisture con- 60 tained in the original sawdust, or int-roduced with the steam, exists at this temperature la rgeiy or wholly as vapor, which permeates the wood and fills the pores .and interstices thereof; and the-immediate effect of the introduction of the cold hydrolyzing and thereby to avoid' l charged from above upon the surfacel of the The di-4 agent-is' to bring about a partial'orcomplete lcondensation of this Vapor, 'with the result that a partial vacuum' is formed within the' digester, the-effect being to secure a deeper,

more intimate, and more rapid penetration of the hydrolyzing agent into the substance .of the particles to be converted. Further- "more, the conditions render it possible to vsecure a very perfect adnii'xtu're of the hydrolyzing agei'it with the material to be converted ,since the hydrolyzing agent is .dis-

sawdust, which, under the 'continued rota? tion of the digester, is caused to iiow or fally in a continuous'stream past the spray-nozzle 314e.` By proceeding as above I found it possible to secure a highly effective and 'inti-- mate'distribution of lthe hydrolizing agent through the sawdust, and I have further found that. this intimate distribution results ina material increase in the percentage of fernieutable sugars yielded by the subsequent digestion.v

Preferablytlie hydrolyzing agent is Vintroduced as an aqueous solution, as for example a solution of sulfuric, sulfurous or hydrochloric acid, at normal or lower -ten'iperatures. The amount of such solution is preferably sufficient to bring the acid concentration, based upon the total moisturecontent of the material, to 0.2-0.5 per cent. VVhenan acid solution is introduced as above described at-a temperature materially below that of the wood-waste, it is possible that a materially-increased percentage of liquid may be supplied to the charge witliout saturating it. tothe limit of its absorptive capacity, by reason ofthe deeper penetration obtained. It is regarded as important that the total liquid-content of, the charge, after the introduction .of the hydrolyzing agent, should be less than is required for its complete saturation, in order that the mass may retain its open, permeable and abserptire condition throughout the subsequent steaming for the production of fernicntable sugars; and a primary purpose of the described treatment is to secure the' deep penetration of a limited proportion of a hydrolizing agent, as distinguished from the maximum sa'turation of the material with the conrerting agent. If the acid solution is. to be introduced undei a` low hydrostatic head, it is necessary ii'rst to relieve the internal steam-pressure; or this steam-pressure may' be maintained, the hydrolizingagent, either-as gas or liquid, being forced into the digester at a. corresponding pressure. In either case the condensation of steam willresult in a rapid fall of the internal pressure. and preferably but not necessarily the conditions are so adjusted thatthe pressure within the digester will fall to a vpoint below atmospheric. 'Afterapart orl all of the hydrolizing agenthas been introduced int-o version, `for a suitable time. rule, in the case of sawdust from coniferous the digester and thoroughly incorporated with the charge, lt ainfis again admitted through the pi and the teinperatuie maintained at a de ice proper for the con- As a general Woods, a temperature oi 275 to 32501) maintained for thirty to forty-tive minutes, will suffice. -The steam is then blown ott' and the digested material is leachedfor the extraction of -'fermentable sugars. The conditions of-the process are such that. the die gestedimateria'l is relatively hard, granular and non-absorptive, which qualities permitthej leaching to be quickly effected 'in diffusion apparatus of standard ty e. The resulting solution may vtherea ter be termented and .distilled for the recover cohol in accordance with know methods.

In case ,-1

plurality ot' digesters are .op-

erated, it i's'fpreferred to blow ofi'Y the steam either at--theclose ofthe digestion or follow# ingther-distillation step, into another digester which has been freshly charged. This isaccomplished by opening theyalve 19, When the steam, together Wit-h any volatile matters carried thereby, Will ass through the pipes 18 and 15, and conduit 14.tlowing l,thenceto other digesters through/the inlet- 30 pipe 16 thereof. If desire-d a portion of the vapors may bev-discharged into `the air vthrough the blow-off cock 4 and pipe 5, in

order to economize time yor to avoid the gradual accumulation, in successively-oper-4 ated digest'ers, of such volatile products as may be objectionable either in the digestion or 'inthe subsequent fermentation. lnl case non-resinous Woo'd's aretreated the step of distillation is ofcourse omitted but the operation may be otherwise essentially asa-bo'lve described. The preliminary steainingzot the Wood is advantageous in any case,'in con` junction with the-supply of the hydrolyzing agent ata lower temperature, as assuring the increased penetration above described.

It is to be understood that the conditions above recited relating to the nature and proportion of hydrolyzing agent used,the teni- -peratures and pressures employed, and the time of the operation, are to be regarded as illustrative, and may be varied Within rather Wide limits, depending upon `the character of the raw material, the scale ot operations,

V and other factors. Furthermore, the conditions, as regards concentration and quantity of acid. time and temperature of heating', are to a'I considerable degree convertible tactors, and inaytherefore be varied with nin-- tua-l correlation Within comparatively wide limits. i

The process herein referred to is described in my copending application Ser. llo. 674,166, tiled January 29, 1912.

I claimf 1 Apparatus for treating ligno-cellulose or. the like, comprising a digester mounted for rotation, means orlieating th'efco'ntents thereof, and means operable duriiiglthe ro tation of the digestei tor n'ithdranfingthe vapors trom the digester and for distributing a hydrolyzing agent uponthc surface of' the charge. l y

2. Apparatus for treating lignolcellulose or the like, comprisinga` rligest'e'rl mountedr torrotation, means 'for introdi'icing steam thereinto, and a lixcd conduit extending into the vapor space ot' the digester for distributing a hydi-'olyzing agentI upon the surface of thecharge', said means for introducing steam and hydrolyzing agent operable during the' rotation of the digester.

3; Apparatus for `treating ligno-cellulose or the like, comprising a digestei' mounted for rotation, means for introducing steam thcreinto, means for withdrawing 'vapors from the-digester, and means extending into the vapor space of the digcsteii tor distributing a hydrolyzing a gent upon the surface of' the charge, all of said means operablcrluring the rotation of the digester. i

vel. Apparatus for treating liguri-cellulose or the like, comprising a digestei' mounted for rotation, a fixed pipeor 4conduit extending axially therethrough and having non communicating perforate and iinpertorate sections, a steam-supply connection to the perforate section, and an eduction pipe extending into the vapor space of the digester and communicating with the `imperforate section. y,

Apparatus for treating ligno-cellulose or the like, coniprisiiig a digester mounted for rotation, a fixed pipe or conduit extend ing axially therethrough and havingnon- `communicating perforate and` imperorate sections, a steanrsupply connection'to the pertorate section. and an eduction pipe for Vthe axial pipe and communicating with the iinper'i'foi'ate section theroot.

7. Mn'iaratus for treating ligno-ccllulose or the like, comprising a digester mounted 'for rotation.y a fixed pipe or conduit extendingl axialli therethrough and having noncommunicating perfor-ate and iinperforate sectionss a steamsupply connection to the perforate section, and an'eduction pipe for vapors extendmg upwardly at an angle to the vertieal into the va'por space of the digester and opening thereinto, said eduction pipe supportedfby the'aXial pipeand communieating with the.. imperforate section thereof. l 'i "8. Apparatus for treating ligno-cellulose or the like, comprising'a digester mounted for rotation, a fixed pipe or conduit 'extending'a-Xially therethrough and having noncoinmunicating' perforate and imperforate' Sections, a Steam-supply'connection -to the perforate seetion,`and an eduction pipe for vapors arched upwardly-at an angle tothe lverticalinto the vapor space of the digester and opening thereinto, said eduction pipesupported at -both ends by the' axial'v pipe' and communicating with the imperforate 'section thereof.

9. vApparatus for treating ligne-cellulose or the like, comprising 'a digester mounted for rotation, a fixed pipe or conduit extending axially 4therethrough and having nonvcommunieating perforate and 'imperforate sections, ay steam-supply connection lto the perforate section, an eduction pipe extending -into the Vapor-space ofthe digesterand communicating withA the imperforate. section, and -a supply connection for hydrolyzing agent supportedby said Vapor-eduction pipe'. i 1Q. Apparat-us fortreat-ingligne-cellulose or. the like', comprising a; digester mounted for rotation, a fixed pipe or conduit"'ex tend v ing' axially therethrough andhavingA non- "commnnic'a-ting --perforate and imprforate sections, a steam-supply'connection to the p erforate section, an eduction pipe extending into the vapor spaoe'of the digester and communicating 'with' the imperforate' section, `and a supplyrconnection for hydrolyzing agent Within said 'vapor-eduction pipe.

11; Apparatus for treating lignecellulose or the like, comprising a digester' mounted' for rotation, a xed pipev or conduit extendingA axially therethrough and 'having non'- conimunicating perforate and imperforate sections, a ,steam-supply connection to the',

perforate section, an eduction pipe orj vapors arched upwardly into the vapor space of the digester and opening thereinto, said eduotion pipe supported at both ends by the-axial pipe and communicating lwith ,the imperforatesection thereof, and a supply connectionfor fhyd'rolyzing agentl supported by said vapor-eduction pipe.. X i

12. Apparatus for treatinghgno-celliilos or the like, comprising 'a digeste'r mounttf vfor rotation, a fixed pipe or conduit extend-;

ing' axially therethrough and having non# f communicating perforate andjimperforate sections, a steam-supply connection 'to .the perforat'e section, 'an eductionJy pipe for vapors arched upwardly into thyapor lspace of the digester and openingthereinto, said eduction pipe supported at both ends 'by connection forl liydrolyzing agent Within said vapor-eductlon "pipe.

1S. Apparatus for treating ligne-.cellulose or the like, comprisvin for rotation, and a fixed vapor-eduction pipe4 a digester mounted thgtreim'saidfpipe extending into the Vapor space of the di'gester at an angle to the' 14. Apparatus for treating lignofcellulose the axial pipe and communicating with the viin-.perforatesection thereof, and a supply er. the like, comprising -a 'digester mounted for rotation, a fixedvapor-eduction pipe therein, said pi'e extending into the vapor space of the digester at an angle to the vertical, and a supply conneetionforliydrolyzing agent supported by said vapor=educ tion pipe. y

15. Apparatusor treating ligne-cellulose or'the like, comprising a digester mounted for rotation,'-a fixed' vapor-.eduction pipe therein, saidpipe extending intofthe vapor- ,space of--the digester"at a r1ght angle to the surface' of the mat er1al there1n, and a.

supply connection' for hydrolyzing4 agent supported by said vapor-educton' pipe.

"16. Apparatus'4 foiltreating ligno'cell'ulose 'or the like, eomprising'a digestvermountedfor rotation, a fixed va-pvor-eduction pipe i thereim-and a supply'connection for hydro-- lyzingagent supported said va]g or ,edue.

tion' pipe. 

